CN107620057B - A kind of application method of the phosphating solution for metal processing - Google Patents

A kind of application method of the phosphating solution for metal processing Download PDF

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CN107620057B
CN107620057B CN201711110115.6A CN201711110115A CN107620057B CN 107620057 B CN107620057 B CN 107620057B CN 201711110115 A CN201711110115 A CN 201711110115A CN 107620057 B CN107620057 B CN 107620057B
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phosphatization
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董晓娜
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/40Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
    • C23C22/44Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides

Abstract

The invention discloses a kind of application method of phosphating solution, wherein phosphatization pre-treatment and phosphorating treatment, wherein phosphatization pre-treatment specifically includes that 1) oil removing;2) alkali cleaning;3) pickling;4) wash and etc., the phosphorating treatment includes: that phosphating solution is directly uniformly brushed to one layer of phosphatization liquid film on workpiece using acidproof brush, or one layer of phosphatization liquid film is sprayed using spray gun, or carry out immersion treatment, then dry, workpiece surface formed phosphating coat compact crystallization, phosphatization surface without dust, highlight phenomenon generate, film layer itself reaches technique requirement without brittleness.

Description

A kind of application method of the phosphating solution for metal processing
Technical field
The present invention relates to a kind of phosphating solutions, and it is parkerized to be suitable for metal works japanning front surface more particularly, to one kind Phosphating solution and preparation method thereof, while also disclosing the application method of the phosphating solution.
Background technique
Phosphatization is common pretreatment technology, should belong to chemical conversion film process in principle, is mainly used in steel surface Phosphatization, non-ferrous metal (such as aluminium, zinc) part can also apply phosphatization.The purpose of phosphatization mainly provides protection to parent metal, one Determine to prevent metal to be corroded in degree;For preceding bottoming of painting, the adhesive force and anti-corrosion capability of paint film layer are improved;It is cold in metal Play antifriction lubrication in processing technology.The phosphorating treatment of metal is steel in compositions such as dihydric phosphate, oxidant, auxiliary agents Processing is carried out in phosphating solution and in the process of several microns of thick phosphating coats of its Surface Creation, including zinc system zinc cathode, manganese systems and iron The types such as system.Phosphating coat is mainly used as the bottom of coating, lubricant layer and metal surface protection layer when metal is cold worked etc., can To play antirust, anti-attrition is wear-resisting, and lubrication promotes a variety of effects such as coating and metallic substrates adhesive force.Phosphatization can significantly improve painting Layer adhesive force, protective capacities, be guarantee coating quality key technology, be automobile, household electrical appliances, machinery production necessary technique. The phosphorization technology being commonly used is zinc system middle temperature phosphating, and phosphatization temperature is high, is also easy to produce acid mist, and tank liquor is unstable, is sunk simultaneously Slag is more, and phosphating coat is thick and heavy, and the adhesive force of film is lower after coating, and corrosion resistance is also poor, used nitrite and a huge sum of money Belong to ionic soil environment.In recent years, with the progress of phosphorization technology, both at home and abroad just in active development quick phosphorization process, phosphorus Change temperature is low, less energy consumption, sediment is few, crystal grain is thin, film is thin, the adhesive force of film and corrosion resistance improve a lot.Country's phosphorus at present Change technology common problem is: phosphatization temperature is high, phosphating solution service life is short, washing difficulty is big and causes water pollution The problems such as, not only the resources such as burden but also a large amount of water of consumption, phosphate are brought to environmental improvement.
From the forming process principle of phosphating coat it is found that the acidity of solution, oxidant, catalyst are the weights for influencing phosphatization speed Factor is wanted, conclusive effect is played to phosphatization quality, therefore the configuration and adjustment of phosphating solution constituent content must highly be given Pay attention to, the component configuration of especially oxidant, catalyst plays key effect, and vast scientific research and enterprise are also actively to oxidation Agent, the formula preparation of catalyst carry out experimental study.
Summary of the invention
The purpose of the present invention is to provide a kind of not only with film forming is quick, film adhesion is strong, corrosion resistance is good, can pass through The advantages that being operated, is easy to operate, is at low cost is brushed or sprayed, and is suitable for the phosphating solution of large-scale workpiece or outdoor equipment And preparation method thereof.
The raw material composition of the phosphating solution is by weight are as follows: and 80-150 parts of zinc dihydrogen phosphate, 10-30 parts of zinc oxide, phosphoric acid 30- It is 50 parts, 2-5 parts of manganese carbonate, 2-4 parts of prodan, 1-5 parts of hydroxyl sulfate, 4-8 parts of triazole compounds, 2-3 parts of sodium citrate, more 10-15 parts of Quadrafos, 1-3 parts of sodium fluoride, 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, 1-2 parts of potassium chlorate, hexa-methylene 1-3 parts of tetramine, 3-5 parts of ring sodium trimetaphosphate, preparation method are as follows: will first be aoxidized in acid-resistant container or Phosphating Slot with suitable quantity of water 10-30 parts of zinc are completely dissolved, and 30-50 parts of phosphoric acid are added after being sufficiently stirred and continues to stir, and it is small to be heated to 100-120 DEG C of heat preservation 2 Shi Jinhang sufficiently reacts, zinc dihydrogen phosphate 80-150 parts, 2-5 parts of manganese carbonate of addition after sufficiently reacting, and 2-4 parts of prodan, 1-5 parts of hydroxyl sulfate, 4-8 parts of triazole compounds, 1-3 parts of sodium fluoride, 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, potassium chlorate 1-2 parts, 1-3 parts of hexa, 3-5 parts of ring sodium trimetaphosphate stir evenly, be eventually adding 10-15 parts of polyphosphate, It 2-3 parts of sodium citrate, then adds suitable quantity of water and carries out pH value adjustment after mixing evenly.
It is had the advantage that compared to existing phosphating solution composition and preparation method, above-mentioned phosphating solution,
1) oxidant, the promotor used includes manganese carbonate, prodan, hydroxyl sulfate, triazole compounds, citric acid Sodium, polyphosphate, sodium fluoride, ammonium peroxydisulfate, sodium molybdate, potassium chlorate, hexa, ring sodium trimetaphosphate, through trying Verifying, component configuration can make the spies such as the phosphating solution being prepared into out film forming is quick, film adhesion is strong, corrosion resistance is good Point;
2) for example, the usage amount of phosphoric acid can be reduced to the full extent using a small amount of appropriate amount of components of hydroxyl sulfate, thus It reduces cost and reduces pollution, make Fe be oxidized to Fe more importantly it can accelerate substrate corrosion reaction speed2+Ferrous iron Ion promotes to dissociate a large amount of PO4 in phosphating solution to rapidly deplete a large amount of hydrogen ions3-, with Zn2+, Fe2+Reaction and in workpiece Phosphating coat nucleus and fast-growth at the fast deposition of surface;
3) not only may be used using the configuration of activation promotor of sodium fluoride 1-3 parts, 2-4 parts of prodan, 1-5 parts of hydroxyl sulfate To accelerate phosphatization nucleus to be formed, so that nucleus densification corrosion resistance enhances, the phosphatization speed of phosphating solution entirety may also speed up, promote It is careful into phosphate coating;
4) oxidant used is formed by components such as 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, 1-2 parts of potassium chlorate, is risen Have to have between very strong oxidisability, especially sodium molybdate and phosphating solution main component in an acidic solution and coordinates effect well It answers, can effectively reduce treatment temperature, improve film forming speed, corrosion inhibiter can also be played the role of and reduce phosphatization film thickness;
5) suitable hexa is added, mainly uses as buffer metal material corrosion agent, can also rise To the effect to phosphating solution pH value adjustment;Suitable ring sodium trimetaphosphate is added, its role is to generate complex chemical compound to divide Heavy metal that may be present is solved, dispersing agent and stabilizer are used as;
6) suitable triazole compounds are added, mainly it can occur absorption in metal surface or form complex, in molybdenum The new adsorption layer for forming heterocyclic compound on the passivating film that sour sodium and metal are formed again, constitutes the change of one layer of three-dimensional net structure Compound film, absorption of the heterocyclic compound at micropore effectively plugs the diffusion admittance of metal ion, while also preventing CI- It is permeated into metal, to significantly reduce the corrosion rate to metal works with sodium molybdate component;
7) being added polyphosphate 10-15 parts, 2-3 parts of sodium citrate in the final stage for preparing phosphating solution can be abundant Its effect as nucleus regulator and slag reduction agent is played, experiment proves that, compared to conventional art, this method can reduce phosphorus Slugging forms 5-10% or more.
It should be noted that oxidant, promotor are to realize low temperature phosphor conditio sune qua non, solution acidity, oxygen Agent, catalyst are an important factor for influencing phosphatization speed, to play conclusive effect, oxidant, promotor to phosphatization quality The low then phosphatization speed of concentration it is slow, it is too low, do not form a film, otherwise excessive concentration, phosphatization speed is fast, it may appear that reaction process is too fast, It is not easy situations such as forming suitable thickness, therefore the formation of said components allocation ratio is determined and needed by creative consideration and examination Verifying could be determined finally.
The invention also discloses a kind of application methods of phosphating solution, including workpiece to be processed is carried out phosphatization pre-treatment and phosphorus Change two steps of processing,
Wherein phosphatization pre-treatment specifically includes that
1) oil removing: workpiece to be processed is immersed in acetone soln, cleans 10-15min using ultrasonic cleaner, will be oily Dirt is sufficiently cleaned;
2) alkali cleaning: workpiece to be processed is immersed in thermostat water bath and is kept for 60 DEG C, embathes 15-20min, alkali wash water is The Na of 50g/L2PO4, 50g/L Na2CO3And the N of 20g/L2SiO3Mixed solution, pH value 7, thermostat water bath keep temperature Degree is acted at 60 DEG C, time about 15-20min;
3) pickling: pickling solution used is the H of 150mL/L2SO4, 50mL/L HF and 30mL/L triethanolamine mixing it is molten Liquid controls temperature at 25 DEG C or so, and pickling time is about 2min;
4) it washes: first being rinsed well with deionized water, but still remained at body surface especially surface concave, aperture position Acid solution is easy to get rusty again, needs to be neutralized after water washing, main molten using the sodium carbonate of 20-40g/L Liquid handles 1-2min, then carries out secondary deionized water flushing, stand-by after cold wind drying;
The phosphorating treatment includes: that gained phosphating solution will be directly prepared according to 1 method of the claims using acidproof brush One layer of phosphatization liquid film is uniformly brushed on workpiece, perhaps spray one layer of phosphatization liquid film using spray gun or carries out immersion treatment, so Afterwards dry, workpiece surface formed phosphating coat compact crystallization, phosphatization surface without dust, highlight phenomenon generate, film layer itself Without brittleness, that is, reach technique requirement.
Compared with prior art, it is the advantages of phosphating solution of the present invention, with film forming is quick, film adhesion is strong, anti-corrosion Property is good, can be by brushing or spraying the advantages that being operated, is easy to operate, at low cost, and the phosphating solution of the preparation not only reduces Phosphating solution sediment guarantees the quality of phosphating coat, and even film layer is fine and smooth, and have a wide range of application model, at low cost, easy to use, is conducive to Industrialized production.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The raw material composition of the phosphating solution is by weight are as follows: and 80-150 parts of zinc dihydrogen phosphate, 10-30 parts of zinc oxide, phosphoric acid 30-50 parts, 2-5 parts of manganese carbonate, 2-4 parts of prodan, 1-5 parts of hydroxyl sulfate, 4-8 parts of triazole compounds, sodium citrate 2-3 Part, 10-15 parts of polyphosphate, 1-3 parts of sodium fluoride, 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, 1-2 parts of potassium chlorate, six is sub- 1-3 parts of tetramine, 3-5 parts of ring sodium trimetaphosphate, preparation method are as follows: first will with suitable quantity of water in acid-resistant container or Phosphating Slot 10-30 parts of zinc oxide are completely dissolved, and 30-50 parts of phosphoric acid are added after being sufficiently stirred and continues to stir, and are heated to 100-120 DEG C of heat preservation It is sufficiently reacted within 2 hours, zinc dihydrogen phosphate 80-150 parts, 2-5 parts of manganese carbonate, prodan 2-4 is added after sufficiently reacting Part, 1-5 parts of hydroxyl sulfate, 4-8 parts of triazole compounds, 1-3 parts of sodium fluoride, 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, chloric acid 1-2 parts of potassium, 1-3 parts of hexa, 3-5 parts of ring sodium trimetaphosphate stir evenly, and are eventually adding polyphosphate 10-15 Then part, 2-3 parts of sodium citrate add suitable quantity of water and carry out pH value adjustment after mixing evenly.
It is had the advantage that compared to existing phosphating solution composition and preparation method, above-mentioned phosphating solution,
1) oxidant, the promotor used includes manganese carbonate, prodan, hydroxyl sulfate, triazole compounds, citric acid Sodium, polyphosphate, sodium fluoride, ammonium peroxydisulfate, sodium molybdate, potassium chlorate, hexa, ring sodium trimetaphosphate, through trying Verifying, component configuration have special role, can make the phosphating solution being prepared into out film forming quickly, film adhesion it is strong, The features such as corrosion resistance is good;
2) for example, the usage amount of phosphoric acid can be reduced to the full extent using a small amount of appropriate amount of components of hydroxyl sulfate, thus It reduces cost and reduces pollution, make FE be oxidized to Fe more importantly it can accelerate substrate corrosion reaction speed2+Ferrous iron Ion promotes to dissociate a large amount of PO4 in phosphating solution to rapidly deplete a large amount of hydrogen ions3-, with Zn2+, Fe2+Reaction and in workpiece Phosphating coat nucleus and fast-growth at the fast deposition of surface;
3) not only may be used using the configuration of activation promotor of sodium fluoride 1-3 parts, 2-4 parts of prodan, 1-5 parts of hydroxyl sulfate To accelerate phosphatization nucleus to be formed, so that nucleus densification corrosion resistance enhances, the phosphatization speed of phosphating solution entirety may also speed up, promote It is careful into phosphate coating;
4) oxidant used is formed by components such as 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, 1-2 parts of potassium chlorate, is risen Have to have between very strong oxidisability, especially sodium molybdate and phosphating solution main component in an acidic solution and coordinates effect well It answers, can effectively reduce treatment temperature, improve film forming speed, corrosion inhibiter can also be played the role of and reduce phosphatization film thickness;
5) suitable hexa is added, mainly uses as buffer metal material corrosion agent, can also rise To the effect to phosphating solution pH value adjustment;Suitable ring sodium trimetaphosphate is added, its role is to generate complex chemical compound to divide Heavy metal that may be present is solved, dispersing agent and stabilizer are used as;
6) suitable triazole compounds are added, mainly it can occur absorption in metal surface or form complex, in molybdenum The new adsorption layer for forming heterocyclic compound on the passivating film that sour sodium and metal are formed again, constitutes the change of one layer of three-dimensional net structure Compound film, absorption of the heterocyclic compound at micropore effectively plugs the diffusion admittance of metal ion, while also preventing CI- It is permeated into metal, to significantly reduce the corrosion rate to metal works with sodium molybdate component;
7) being added polyphosphate 10-15 parts, 2-3 parts of sodium citrate in the final stage for preparing phosphating solution can be abundant Its effect as nucleus regulator and slag reduction agent is played, experiment proves that, compared to conventional art, this method can reduce phosphorus Slugging forms 5-10% or more.
It should be noted that oxidant, promotor are to realize low temperature phosphor conditio sune qua non, solution acidity, oxygen Agent, catalyst are an important factor for influencing phosphatization speed, to play conclusive effect, oxidant, promotor to phosphatization quality The low then phosphatization speed of concentration it is slow, it is too low, do not form a film, otherwise excessive concentration, phosphatization speed is fast, it may appear that reaction process is too fast, It is not easy situations such as forming suitable thickness, therefore the formation of above-mentioned allocation ratio is needed by creative consideration and tested through overtesting Card could be determined finally.The total acidity TA of phosphating solution is 50-90 point, and acidity ratio (TA/FA) is in the range of 5-15 point.
Following embodiment and correlation data are provided to prove the technical effect of the application
Embodiment 1
The raw material composition of the phosphating solution is by weight are as follows: and 100 parts of zinc dihydrogen phosphate, 15 parts of zinc oxide, 0 part of phosphatase 24, carbon 2 parts of sour manganese, 2 parts of prodan, 4 parts of hydroxyl sulfate, 4 parts of triazole compounds, 2 parts of sodium citrate, 10 parts of polyphosphate, fluorination 2 parts of sodium, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 1 part of potassium chlorate, 1 part of hexa, 3 parts of ring sodium trimetaphosphate,
Preparation method are as follows: be first completely dissolved 15 parts of zinc oxide with suitable quantity of water in acid-resistant container or Phosphating Slot, sufficiently 0 part of phosphatase 24 is added after stirring to continue to stir, and is heated to 100-120 DEG C of heat preservation and is sufficiently reacted for 2 hours, to sufficiently react Addition 100 parts of zinc dihydrogen phosphate, 2 parts of manganese carbonate afterwards, 2 parts of prodan, 4 parts of hydroxyl sulfate, 4 parts of triazole compounds, sodium fluoride 2 Part, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 1 part of potassium chlorate, 1 part of hexa, 3 parts of ring sodium trimetaphosphate stir evenly, It is eventually adding 10 parts of polyphosphate, 2 parts of sodium citrate, suitable quantity of water is then added and carries out pH value adjustment after mixing evenly i.e. It can.
Embodiment 2
The raw material composition of the phosphating solution is by weight are as follows: and 100 parts of zinc dihydrogen phosphate, 15 parts of zinc oxide, 0 part of phosphatase 24, carbon 2 parts of sour manganese, 3.5 parts of prodan, 4 parts of hydroxyl sulfate, 4 parts of triazole compounds, 2 parts of sodium citrate, 10 parts of polyphosphate, fluorine Change 3 parts of sodium, it 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 2 parts of potassium chlorate, 1 part of hexa, 3 parts of ring sodium trimetaphosphate, can To find out, compared to embodiment 1, activator component configuration is increased.
Preparation method are as follows: be first completely dissolved 15 parts of zinc oxide with suitable quantity of water in acid-resistant container or Phosphating Slot, sufficiently 0 part of phosphatase 24 is added after stirring to continue to stir, and is heated to 100-120 DEG C of heat preservation and is sufficiently reacted for 2 hours, to sufficiently react 100 parts of zinc dihydrogen phosphate, 2 parts of manganese carbonate are added afterwards, 3.5 parts of prodan, 4 parts of hydroxyl sulfate, 4 parts of triazole compounds, is fluorinated 3 parts of sodium, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 2 parts of potassium chlorate, 1 part of hexa, 3 parts of ring sodium trimetaphosphate stirrings are equal It is even, it is eventually adding 10 parts of polyphosphate, 2 parts of sodium citrate, suitable quantity of water is then added and carries out pH value adjustment after mixing evenly ?.
Embodiment 3
The raw material composition of the phosphating solution is by weight are as follows: and 100 parts of zinc dihydrogen phosphate, 15 parts of zinc oxide, 0 part of phosphatase 24, carbon 2 parts of sour manganese, 2 parts of prodan, 4 parts of hydroxyl sulfate, 6 parts of triazole compounds, 2 parts of sodium citrate, 10 parts of polyphosphate, fluorination It 2 parts of sodium, 2 parts of ammonium peroxydisulfate, 8 parts of sodium molybdate, 2 parts of potassium chlorate, 1 part of hexa, 3 parts of ring sodium trimetaphosphate, can be with Find out, compared to embodiment 1, increases oxidant constituents configuration.
Preparation method are as follows: be first completely dissolved 15 parts of zinc oxide with suitable quantity of water in acid-resistant container or Phosphating Slot, sufficiently 0 part of phosphatase 24 is added after stirring to continue to stir, and is heated to 100-120 DEG C of heat preservation and is sufficiently reacted for 2 hours, to sufficiently react Addition 100 parts of zinc dihydrogen phosphate, 2 parts of manganese carbonate afterwards, 2 parts of prodan, 4 parts of hydroxyl sulfate, 6 parts of triazole compounds, sodium fluoride 2 Part, 2 parts of ammonium peroxydisulfate, 8 parts of sodium molybdate, 2 parts of potassium chlorate, 1 part of hexa, 3 parts of ring sodium trimetaphosphate stir evenly, It is eventually adding 10 parts of polyphosphate, 2 parts of sodium citrate, suitable quantity of water is then added and carries out pH value adjustment after mixing evenly i.e. It can.
Embodiment 4
The raw material composition of the phosphating solution is by weight are as follows: and 100 parts of zinc dihydrogen phosphate, 15 parts of zinc oxide, 0 part of phosphatase 24, carbon 2 parts of sour manganese, 2 parts of prodan, 4 parts of hydroxyl sulfate, 4 parts of triazole compounds, 2 parts of sodium citrate, 10 parts of polyphosphate, fluorination It 2 parts of sodium, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 1 part of potassium chlorate, 2 parts of hexa, 5 parts of ring sodium trimetaphosphate, can be with Find out, compared to embodiment 1, has adjusted hexa and the configuration of ring sodium trimetaphosphate component.
Preparation method are as follows: be first completely dissolved 15 parts of zinc oxide with suitable quantity of water in acid-resistant container or Phosphating Slot, sufficiently 0 part of phosphatase 24 is added after stirring to continue to stir, and is heated to 100-120 DEG C of heat preservation and is sufficiently reacted for 2 hours, to sufficiently react Addition 100 parts of zinc dihydrogen phosphate, 2 parts of manganese carbonate afterwards, 2 parts of prodan, 4 parts of hydroxyl sulfate, 4 parts of triazole compounds, sodium fluoride 2 Part, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 1 part of potassium chlorate, 2 parts of hexa, 5 parts of ring sodium trimetaphosphate stir evenly, It is eventually adding 10 parts of polyphosphate, 2 parts of sodium citrate, suitable quantity of water is then added and carries out pH value adjustment after mixing evenly i.e. It can.
Embodiment 5
The raw material composition of the phosphating solution is by weight are as follows: and 80 parts of zinc dihydrogen phosphate, 10 parts of zinc oxide, 30 parts of phosphoric acid, carbon 2 parts of sour manganese, 2 parts of prodan, 2.5 parts of hydroxyl sulfate, 6 parts of triazole compounds, 2 parts of sodium citrate, 10 parts of polyphosphate, fluorine 1.5 parts of sodium of change, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 2 parts of potassium chlorate, 2 parts of hexa, 4 parts of ring sodium trimetaphosphate,
Preparation method are as follows: be first completely dissolved 10 parts of zinc oxide with suitable quantity of water in acid-resistant container or Phosphating Slot, sufficiently 30 parts of phosphoric acid are added after stirring to continue to stir, and are heated to 100-120 DEG C of heat preservation and are sufficiently reacted for 2 hours, to sufficiently react Addition 80 parts of zinc dihydrogen phosphate, 2 parts of manganese carbonate afterwards, 2 parts of prodan, 2.5 parts of hydroxyl sulfate, 6 parts of triazole compounds, sodium fluoride 1.5 parts, 2 parts of ammonium peroxydisulfate, 5 parts of sodium molybdate, 2 parts of potassium chlorate, 2 parts of hexa, 4 parts of ring sodium trimetaphosphate stirrings are equal It is even, it is eventually adding 10 parts of polyphosphate, 2 parts of sodium citrate, suitable quantity of water is then added and carries out pH value adjustment after mixing evenly ?.
The phosphating solution that above-described embodiment 1-5 is obtained carries out phosphorating treatment, environmental parameter: room temperature 20 to same metal works DEG C, normal pressure, humidity 70%, efficacy parameter is compared as follows:
Meanwhile only paying attention to production link in the industrial production in China at present and ignoring practice and operate construction application, so that good The application that cannot get well of product, and then cannot achieve corresponding technical effect, therefore the invention also discloses a kind of phosphating solutions Application method, including workpiece to be processed is subjected to two steps of phosphatization pre-treatment and phosphorating treatment, phosphatization pre-treatment mainly wraps It includes:
1) oil removing: workpiece to be processed is immersed in acetone soln, cleans 10-15min using ultrasonic cleaner, will be oily Dirt is sufficiently cleaned;
2) alkali cleaning: workpiece to be processed is immersed in thermostat water bath and is kept for 60 DEG C, embathes 15-20min, alkali wash water is The Na of 50g/L2PO4, 50g/L Na2CO3And the N of 20g/L2SiO3Mixed solution, pH value 7, thermostat water bath keep temperature Degree is acted at 60 DEG C, and time about 15-20min, the purpose using ultrasonic cleaning and alkali liquor oil removing is to preferably remove Cold working clast, grease and the dirt of specimen surface adherency;
3) pickling: pickling solution used is the H of 150mL/L2SO4, 50mL/L HF and 30mL/L triethanolamine mixing it is molten Liquid controls temperature at 25 DEG C or so, and pickling time is about 2min.The pickling solution is sour based on sulfuric acid, cooperates with hydrofluoric acid and three Ethanol amine addition is fused, is mainly used for the processing of high-alloy steel and stainless steel using the acid solution of the formulation components, can Fast and effeciently remove the oxide of workpiece surface.
4) it washes: first being rinsed well with deionized water, but still remained at body surface especially surface concave, aperture position Acid solution is easy to get rusty again, needs to be neutralized after water washing, main molten using the sodium carbonate of 20-40g/L Liquid handles 1-2min, then carries out secondary deionized water flushing, stand-by after cold wind drying;
The phosphorating treatment includes: that above-described embodiment 1-5 method is directly prepared gained phosphating solution in work using acidproof brush One layer of phosphatization liquid film is uniformly brushed on part, perhaps spray one layer of phosphatization liquid film using spray gun or carries out immersion treatment, is then done It is dry, workpiece surface formed phosphating coat compact crystallization, phosphatization surface without dust, highlight phenomenon generate, film layer itself is without crisp Property, that is, reach technique requirement.
Although the detailed description and description of the specific embodiments of the present invention are given above, it should be noted that We can carry out various equivalent changes and modification to above embodiment according to the concept of the present invention, and generated function is made With still without departing from covered spirit is illustrated when, should all be within protection scope of the present invention.The above, it is only of the invention Preferred embodiment is not intended to limit the invention, to the above embodiments any according to the technical essence of the invention Trickle amendment, equivalent replacement and improvement, all should be included in the scope of protection of the technical solution of the present invention.

Claims (1)

1. a kind of application method of phosphating solution, including workpiece to be processed is subjected to two steps of phosphatization pre-treatment and phosphorating treatment,
Wherein phosphatization pre-treatment specifically includes that
1) oil removing: workpiece to be processed is immersed in acetone soln, using ultrasonic cleaner clean 10-15min, by greasy dirt into Row sufficiently cleaning;
2) alkali cleaning: workpiece to be processed is immersed in thermostat water bath and is kept for 60 DEG C, embathes 15-20min, alkali wash water 50g/L Na2PO4, 50g/L Na2CO3And the N of 20g/L2SiO3Mixed solution, pH value 7, thermostat water bath maintains the temperature at 60 DEG C, time 15-20min;
3) pickling: pickling solution used is the H of 150mL/L2SO4, 50mL/L HF and 30mL/L triethanolamine mixed solution, Temperature is controlled at 25 DEG C, pickling time 2min;
4) it washes: first being rinsed well with deionized water, but in body surface especially surface concave, aperture position still residual acid Liquid is easy to get rusty again, needs to be neutralized after water washing, the main sodium carbonate liquor for using 20-40g/L, 1-2min is handled, secondary deionized water flushing is then carried out, it is stand-by after cold wind drying;The phosphorating treatment includes: using acidproof Brush phosphating solution is directly uniformly brushed to one layer of phosphatization liquid film on workpiece, perhaps using spray gun spray one layer of phosphatization liquid film or Carry out immersion treatment, then dry, the phosphating coat compact crystallization that workpiece surface is formed, phosphatization surface without dust, highlight it is existing As generating, film layer itself reaches technique requirement without brittleness;
The raw material composition of used phosphating solution is by weight are as follows: and 80-150 parts of zinc dihydrogen phosphate, 10-30 parts of zinc oxide, phosphoric acid 30-50 parts, 2-5 parts of manganese carbonate, 2-4 parts of prodan, 1-5 parts of hydroxyl sulfate, 4-8 parts of triazole compounds, sodium citrate 2-3 Part, 10-15 parts of polyphosphate, 1-3 parts of sodium fluoride, 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, 1-2 parts of potassium chlorate, six is sub- 1-3 parts of tetramine, 3-5 parts of ring sodium trimetaphosphate.
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